#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/76/4307617.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_4307617
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         'C14 H22 N6, H2 O'
_chemical_formula_sum            'C14 H24 N6 O'
_chemical_formula_weight         292.39
_chemical_name_systematic
;
 ?
;
_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                91.898(3)
_cell_angle_beta                 99.040(3)
_cell_angle_gamma                117.182(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9700(12)
_cell_length_b                   9.6283(12)
_cell_length_c                   10.6464(14)
_cell_measurement_temperature    180(2)
_cell_volume                     802.00(18)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0827P)²+0.0232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                1811
_reflns_number_total             2778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062093csi20061102_124645_1.cif
_cod_data_source_block           6
_cod_database_code               4307617
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
H1 H 0.584(4) 0.096(3) 0.732(3) 0.044(9) Uiso 1 1 d . . .
H21 H 0.2122 0.1569 0.6048 0.050 Uiso 1 1 d . . .
H22 H 0.3786 0.1258 0.6018 0.050 Uiso 1 1 d . . .
O1 O 0.2463(2) 0.0905(3) 0.5579(2) 0.0500(6) Uani 1 1 d . . .
N1 N 1.0297(3) 0.2926(2) 0.7477(2) 0.0270(6) Uani 1 1 d . . .
N2 N 1.1747(3) 0.2805(3) 0.7411(2) 0.0312(6) Uani 1 1 d . . .
N3 N 0.8160(3) 0.0568(3) 0.8049(2) 0.0300(6) Uani 1 1 d . . .
N4 N 0.7749(3) 0.1120(3) 0.9068(2) 0.0358(6) Uani 1 1 d . . .
N5 N 0.5819(3) 0.1401(3) 0.6618(3) 0.0401(7) Uani 1 1 d . . .
N6 N 0.7705(3) 0.2762(3) 0.5339(2) 0.0347(6) Uani 1 1 d . . .
C1 C 1.3026(3) 0.4160(3) 0.8011(3) 0.0334(7) Uani 1 1 d . . .
C2 C 1.2397(4) 0.5131(3) 0.8463(3) 0.0357(7) Uani 1 1 d . . .
H2 H 1.3057 0.6155 0.8918 0.043 Uiso 1 1 calc R . .
C3 C 1.0658(4) 0.4329(3) 0.8125(2) 0.0303(7) Uani 1 1 d . . .
C4 C 1.4830(3) 0.4467(4) 0.8089(3) 0.0493(9) Uani 1 1 d . . .
H4A H 1.4840 0.3555 0.7662 0.074 Uiso 1 1 calc R . .
H4B H 1.5392 0.4651 0.8990 0.074 Uiso 1 1 calc R . .
H4C H 1.5442 0.5397 0.7666 0.074 Uiso 1 1 calc R . .
C5 C 0.9344(4) 0.4803(3) 0.8339(3) 0.0401(8) Uani 1 1 d . . .
H5A H 0.8754 0.4891 0.7513 0.060 Uiso 1 1 calc R . .
H5B H 0.9897 0.5820 0.8874 0.060 Uiso 1 1 calc R . .
H5C H 0.8515 0.4009 0.8771 0.060 Uiso 1 1 calc R . .
C6 C 0.7470(3) 0.0029(4) 0.9866(3) 0.0370(7) Uani 1 1 d . . .
C7 C 0.7724(4) -0.1188(4) 0.9366(3) 0.0415(8) Uani 1 1 d . . .
H7 H 0.7608 -0.2095 0.9758 0.050 Uiso 1 1 calc R . .
C8 C 0.8172(3) -0.0825(3) 0.8210(3) 0.0338(7) Uani 1 1 d . . .
C9 C 0.8626(4) -0.1666(3) 0.7257(3) 0.0465(9) Uani 1 1 d . . .
H9A H 0.7756 -0.2030 0.6469 0.070 Uiso 1 1 calc R . .
H9B H 0.8681 -0.2572 0.7612 0.070 Uiso 1 1 calc R . .
H9C H 0.9740 -0.0949 0.7064 0.070 Uiso 1 1 calc R . .
C10 C 0.6908(4) 0.0165(4) 1.1091(3) 0.0553(10) Uani 1 1 d . . .
H10A H 0.7285 0.1274 1.1368 0.083 Uiso 1 1 calc R . .
H10B H 0.7410 -0.0268 1.1749 0.083 Uiso 1 1 calc R . .
H10C H 0.5659 -0.0422 1.0959 0.083 Uiso 1 1 calc R . .
C11 C 0.8683(3) 0.1527(3) 0.7022(2) 0.0282(7) Uani 1 1 d . . .
H11 H 0.8898 0.0893 0.6378 0.034 Uiso 1 1 calc R . .
C12 C 0.7283(3) 0.1869(3) 0.6322(3) 0.0300(7) Uani 1 1 d . . .
C13 C 0.8993(4) 0.2841(4) 0.4613(3) 0.0434(8) Uani 1 1 d . . .
H13A H 0.9874 0.2688 0.5169 0.065 Uiso 1 1 calc R . .
H13B H 0.9518 0.3872 0.4303 0.065 Uiso 1 1 calc R . .
H13C H 0.8451 0.2016 0.3882 0.065 Uiso 1 1 calc R . .
C14 C 0.6397(4) 0.3089(4) 0.4632(3) 0.0507(9) Uani 1 1 d . . .
H14A H 0.5516 0.2134 0.4090 0.076 Uiso 1 1 calc R . .
H14B H 0.6916 0.3921 0.4094 0.076 Uiso 1 1 calc R . .
H14C H 0.5878 0.3432 0.5236 0.076 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'
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 112.0(2) . . ?
C3 N1 C11 130.8(2) . . ?
N2 N1 C11 116.67(19) . . ?
C1 N2 N1 104.9(2) . . ?
N4 N3 C8 112.3(2) . . ?
N4 N3 C11 119.9(2) . . ?
C8 N3 C11 127.5(2) . . ?
C6 N4 N3 104.5(2) . . ?
C12 N6 C14 117.1(2) . . ?
C12 N6 C13 123.6(2) . . ?
C14 N6 C13 114.2(2) . . ?
N2 C1 C2 110.6(2) . . ?
N2 C1 C4 119.8(3) . . ?
C2 C1 C4 129.6(3) . . ?
C3 C2 C1 107.1(2) . . ?
C2 C3 N1 105.5(2) . . ?
C2 C3 C5 130.3(3) . . ?
N1 C3 C5 124.2(3) . . ?
N4 C6 C7 110.8(3) . . ?
N4 C6 C10 121.2(3) . . ?
C7 C6 C10 127.9(3) . . ?
C8 C7 C6 106.9(3) . . ?
N3 C8 C7 105.5(3) . . ?
N3 C8 C9 123.5(3) . . ?
C7 C8 C9 131.1(3) . . ?
N3 C11 N1 110.6(2) . . ?
N3 C11 C12 112.9(2) . . ?
N1 C11 C12 113.6(2) . . ?
N5 C12 N6 120.3(3) . . ?
N5 C12 C11 124.3(3) . . ?
N6 C12 C11 115.3(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
N1 C3 1.369(3) . ?
N1 N2 1.370(3) . ?
N1 C11 1.449(3) . ?
N2 C1 1.332(3) . ?
N3 N4 1.364(3) . ?
N3 C8 1.363(3) . ?
N3 C11 1.449(3) . ?
N4 C6 1.332(4) . ?
N5 C12 1.275(3) . ?
N6 C12 1.366(3) . ?
N6 C14 1.456(4) . ?
N6 C13 1.463(3) . ?
C1 C2 1.400(4) . ?
C1 C4 1.494(4) . ?
C2 C3 1.365(4) . ?
C3 C5 1.490(4) . ?
C6 C7 1.395(4) . ?
C6 C10 1.493(4) . ?
C7 C8 1.362(4) . ?
C8 C9 1.493(4) . ?
C11 C12 1.530(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21156065
