#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024324.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_7024324
loop_
_publ_author_name
'Otero, Antonio'
'Lara-Sánchez, Agustín'
'Fernández-Baeza, Juan'
'Martínez-Caballero, Emilia'
'Márquez-Segovia, Isabel'
'Alonso-Moreno, Carlos'
'Sánchez-Barba, Luis F'
'Rodríguez, Ana M'
'López-Solera, Isabel'
_publ_section_title
;
 New achiral and chiral NNE heteroscorpionate ligands. Synthesis of
 homoleptic lithium complexes as well as halide and alkyl scandium and
 yttrium complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              930
_journal_page_last               940
_journal_paper_doi               10.1039/b914966j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C16 H25 N5 S'
_chemical_formula_weight         319.47
_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                89.887(3)
_cell_angle_beta                 83.512(3)
_cell_angle_gamma                75.696(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6457(13)
_cell_length_b                   9.4203(14)
_cell_length_c                   11.1657(17)
_cell_measurement_temperature    180(2)
_cell_volume                     875.2(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      180(2)
_diffrn_measured_fraction_theta_full 0.732
_diffrn_measured_fraction_theta_max 0.732
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4266
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.581279
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.411
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0530
_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)+(0.0818P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                1912
_reflns_number_total             2645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914966j.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024324
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
S1 S 0.27262(10) 0.19623(9) 0.55334(7) 0.0413(3) Uani 1 1 d .
C3 C 0.7241(3) 0.3572(3) 0.8557(2) 0.0259(6) Uani 1 1 d .
C2 C 0.4886(3) 0.1641(3) 0.7168(2) 0.0247(6) Uani 1 1 d .
H2 H 0.5403 0.0818 0.6607 0.030 Uiso 1 1 calc R
C10 C 0.2197(3) 0.1051(3) 0.9596(2) 0.0305(7) Uani 1 1 d .
C5 C 0.7790(3) 0.1694(3) 0.7254(2) 0.0250(6) Uani 1 1 d .
C4 C 0.8487(3) 0.2552(3) 0.7893(2) 0.0275(7) Uani 1 1 d .
H4 H 0.9582 0.2471 0.7886 0.033 Uiso 1 1 calc R
C12 C 0.0754(3) 0.1631(3) 1.0482(3) 0.0385(8) Uani 1 1 d .
H12A H 0.0740 0.2607 1.0740 0.058 Uiso 1 1 calc R
H12B H 0.0791 0.1011 1.1167 0.058 Uiso 1 1 calc R
H12C H -0.0199 0.1650 1.0111 0.058 Uiso 1 1 calc R
C8 C 0.4302(3) -0.0362(3) 0.8503(3) 0.0281(7) Uani 1 1 d .
C9 C 0.3156(3) -0.0374(3) 0.9439(3) 0.0347(7) Uani 1 1 d .
H9 H 0.3035 -0.1180 0.9888 0.042 Uiso 1 1 calc R
C1 C 0.3666(3) 0.2711(3) 0.6485(2) 0.0261(7) Uani 1 1 d .
C13 C 0.2336(3) 0.5429(3) 0.6331(3) 0.0319(7) Uani 1 1 d .
C7 C 0.8538(3) 0.0493(3) 0.6343(3) 0.0354(7) Uani 1 1 d .
H7A H 0.9679 0.0386 0.6220 0.053 Uiso 1 1 calc R
H7B H 0.8097 0.0729 0.5596 0.053 Uiso 1 1 calc R
H7C H 0.8321 -0.0408 0.6629 0.053 Uiso 1 1 calc R
C6 C 0.7357(3) 0.4770(3) 0.9391(3) 0.0369(8) Uani 1 1 d .
H6A H 0.6297 0.5295 0.9722 0.055 Uiso 1 1 calc R
H6B H 0.7886 0.5429 0.8954 0.055 Uiso 1 1 calc R
H6C H 0.7962 0.4355 1.0032 0.055 Uiso 1 1 calc R
C11 C 0.5654(4) -0.1544(3) 0.7928(3) 0.0400(8) Uani 1 1 d .
H11A H 0.5615 -0.1563 0.7073 0.060 Uiso 1 1 calc R
H11B H 0.5565 -0.2471 0.8249 0.060 Uiso 1 1 calc R
H11C H 0.6655 -0.1362 0.8093 0.060 Uiso 1 1 calc R
C15 C 0.2557(4) 0.5520(4) 0.4974(3) 0.0483(9) Uani 1 1 d .
H15A H 0.3624 0.5609 0.4713 0.072 Uiso 1 1 calc R
H15B H 0.1789 0.6359 0.4729 0.072 Uiso 1 1 calc R
H15C H 0.2397 0.4648 0.4617 0.072 Uiso 1 1 calc R
C14 C 0.0639(3) 0.5359(3) 0.6797(3) 0.0444(9) Uani 1 1 d .
H14A H 0.0407 0.4518 0.6443 0.067 Uiso 1 1 calc R
H14B H -0.0108 0.6232 0.6583 0.067 Uiso 1 1 calc R
H14C H 0.0546 0.5283 0.7658 0.067 Uiso 1 1 calc R
C16 C 0.2741(4) 0.6731(3) 0.6907(3) 0.0509(9) Uani 1 1 d .
H16A H 0.2635 0.6646 0.7768 0.076 Uiso 1 1 calc R
H16B H 0.2018 0.7621 0.6696 0.076 Uiso 1 1 calc R
H16C H 0.3825 0.6750 0.6622 0.076 Uiso 1 1 calc R
N2 N 0.5820(3) 0.3376(2) 0.8362(2) 0.0265(6) Uani 1 1 d .
N1 N 0.6173(2) 0.2210(2) 0.75554(18) 0.0233(5) Uani 1 1 d .
N4 N 0.2720(3) 0.1949(2) 0.8809(2) 0.0301(6) Uani 1 1 d .
N3 N 0.4023(3) 0.1052(2) 0.8146(2) 0.0262(6) Uani 1 1 d .
N5 N 0.3482(3) 0.4110(3) 0.6746(2) 0.0266(6) Uani 1 1 d .
H5 H 0.405(3) 0.429(3) 0.728(2) 0.025(8) Uiso 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N2 C3 C4 111.1(2)
N2 C3 C6 120.7(2)
C4 C3 C6 128.2(2)
N3 C2 N1 112.6(2)
N3 C2 C1 108.7(2)
N1 C2 C1 115.8(2)
N4 C10 C9 111.1(3)
N4 C10 C12 120.0(3)
C9 C10 C12 128.9(3)
N1 C5 C4 105.8(2)
N1 C5 C7 124.2(2)
C4 C5 C7 130.0(2)
C5 C4 C3 106.8(2)
C9 C8 N3 105.6(2)
C9 C8 C11 131.6(3)
N3 C8 C11 122.8(2)
C8 C9 C10 106.9(3)
N5 C1 C2 115.4(2)
N5 C1 S1 128.3(2)
C2 C1 S1 116.3(2)
N5 C13 C15 111.1(2)
N5 C13 C14 108.4(2)
C15 C13 C14 111.6(3)
N5 C13 C16 105.3(2)
C15 C13 C16 110.1(2)
C14 C13 C16 110.2(3)
C3 N2 N1 104.7(2)
C5 N1 N2 111.7(2)
C5 N1 C2 128.1(2)
N2 N1 C2 120.1(2)
C10 N4 N3 103.8(2)
C8 N3 N4 112.5(2)
C8 N3 C2 127.7(2)
N4 N3 C2 119.7(2)
C1 N5 C13 130.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C1 1.664(3)
C3 N2 1.329(3)
C3 C4 1.394(4)
C3 C6 1.494(4)
C2 N3 1.441(3)
C2 N1 1.454(3)
C2 C1 1.538(4)
C10 N4 1.337(3)
C10 C9 1.392(4)
C10 C12 1.490(4)
C5 N1 1.365(3)
C5 C4 1.365(4)
C5 C7 1.492(4)
C8 C9 1.358(4)
C8 N3 1.361(3)
C8 C11 1.486(4)
C1 N5 1.317(3)
C13 N5 1.494(4)
C13 C15 1.511(4)
C13 C14 1.517(4)
C13 C16 1.519(4)
N2 N1 1.374(3)
N4 N3 1.369(3)
